# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'W. Levason' _publ_contact_author_email WXL@SOTON.AC.UK _publ_section_title ; Six- and eight-coordinate thio- and seleno-ether complexes of NbF5 and some comparisons with NbCl5 and NbBr5 adducts ; loop_ _publ_author_name 'W. Levason' 'Marek Jura' 'Raju Ratnani' 'Gillian Reid' 'M. Webster' # Attachment 'Nb_all7_b.cif' data_2008mj47 _database_code_depnum_ccdc_archive 'CCDC 723266' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-11-07 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrafluoro-tetrakis(dimethylsulfide-S)niobium(V) hexafluoroniobate(V) ; _chemical_name_common ;tetrafluoro-tetrakis(dimethylsulfide-S)niobium(V) hexafluoroniobate(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H24 F4 Nb S4 1+, F6 Nb 1-' _chemical_formula_sum 'C8 H24 F10 Nb2 S4' _chemical_formula_structural '((C2 H6 S)4 (Nb F4)) (F6 Nb)' _chemical_formula_weight 624.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n c c' _space_group_IT_number 130 _space_group_name_Hall '-P 4a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 12.283(5) _cell_length_b 12.283(5) _cell_length_c 13.860(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2091.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 35419 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 1.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5110 # 0.6501 _exptl_absorpt_correction_T_max 0.7456 # 0.9398 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14628 _diffrn_reflns_av_R_equivalents 0.1505 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1196 _reflns_number_gt 880 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+17.6059P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1196 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.2500 0.7500 0.2500 0.0200(3) Uani 1 4 d S . . Nb2 Nb 0.2500 0.2500 0.40802(9) 0.0248(3) Uani 1 4 d S . . F1 F 0.1474(3) 0.7871(3) 0.1529(3) 0.0241(9) Uani 1 1 d . . . F2 F 0.2500 0.2500 0.2732(6) 0.040(2) Uani 1 4 d S . . F3 F 0.1673(4) 0.3781(4) 0.4107(4) 0.0458(14) Uani 1 1 d . . . F4 F 0.2500 0.2500 0.5451(6) 0.039(2) Uani 1 4 d S . . S1 S 0.04759(15) 0.69194(15) 0.31157(13) 0.0234(4) Uani 1 1 d . . . C1 C -0.0209(6) 0.8203(7) 0.3273(6) 0.0310(18) Uani 1 1 d . . . H1A H -0.0355 0.8528 0.2641 0.047 Uiso 1 1 calc R . . H1B H 0.0253 0.8695 0.3651 0.047 Uiso 1 1 calc R . . H1C H -0.0898 0.8086 0.3614 0.047 Uiso 1 1 calc R . . C2 C 0.0649(7) 0.6484(8) 0.4346(5) 0.0314(19) Uani 1 1 d . . . H2A H 0.1017 0.5777 0.4358 0.047 Uiso 1 1 calc R . . H2B H -0.0066 0.6419 0.4656 0.047 Uiso 1 1 calc R . . H2C H 0.1089 0.7020 0.4695 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0203(4) 0.0203(4) 0.0193(6) 0.000 0.000 -0.0010(7) Nb2 0.0257(5) 0.0257(5) 0.0229(6) 0.000 0.000 0.000 F1 0.025(2) 0.023(2) 0.024(2) 0.0022(17) -0.0041(17) -0.0001(17) F2 0.046(3) 0.046(3) 0.029(5) 0.000 0.000 0.000 F3 0.048(3) 0.037(3) 0.052(3) 0.002(2) 0.008(2) 0.016(3) F4 0.046(3) 0.046(3) 0.024(4) 0.000 0.000 0.000 S1 0.0197(9) 0.0252(10) 0.0252(8) -0.0009(8) 0.0004(8) -0.0009(8) C1 0.024(4) 0.030(4) 0.038(4) 0.001(4) 0.002(3) 0.004(4) C2 0.029(5) 0.039(5) 0.027(4) 0.008(3) 0.006(3) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 F1 1.899(4) 8_665 ? Nb1 F1 1.899(4) . ? Nb1 F1 1.899(4) 7_455 ? Nb1 F1 1.899(4) 2_565 ? Nb1 S1 2.724(2) 7_455 ? Nb1 S1 2.724(2) 2_565 ? Nb1 S1 2.724(2) . ? Nb1 S1 2.724(2) 8_665 ? Nb2 F2 1.869(9) . ? Nb2 F3 1.873(5) 3 ? Nb2 F3 1.873(5) 4 ? Nb2 F3 1.873(5) . ? Nb2 F3 1.873(5) 2 ? Nb2 F4 1.901(8) . ? S1 C2 1.800(7) . ? S1 C1 1.801(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Nb1 F1 100.6(2) 8_665 . ? F1 Nb1 F1 89.8(2) 8_665 7_455 ? F1 Nb1 F1 145.1(2) . 7_455 ? F1 Nb1 F1 145.1(2) 8_665 2_565 ? F1 Nb1 F1 89.8(2) . 2_565 ? F1 Nb1 F1 100.6(2) 7_455 2_565 ? F1 Nb1 S1 139.91(13) 8_665 7_455 ? F1 Nb1 S1 79.81(13) . 7_455 ? F1 Nb1 S1 71.27(13) 7_455 7_455 ? F1 Nb1 S1 74.51(12) 2_565 7_455 ? F1 Nb1 S1 79.81(13) 8_665 2_565 ? F1 Nb1 S1 139.91(13) . 2_565 ? F1 Nb1 S1 74.51(13) 7_455 2_565 ? F1 Nb1 S1 71.27(13) 2_565 2_565 ? S1 Nb1 S1 125.19(8) 7_455 2_565 ? F1 Nb1 S1 74.51(13) 8_665 . ? F1 Nb1 S1 71.27(13) . . ? F1 Nb1 S1 79.81(13) 7_455 . ? F1 Nb1 S1 139.91(13) 2_565 . ? S1 Nb1 S1 67.67(8) 7_455 . ? S1 Nb1 S1 143.48(8) 2_565 . ? F1 Nb1 S1 71.27(13) 8_665 8_665 ? F1 Nb1 S1 74.51(12) . 8_665 ? F1 Nb1 S1 139.91(13) 7_455 8_665 ? F1 Nb1 S1 79.81(13) 2_565 8_665 ? S1 Nb1 S1 143.48(8) 7_455 8_665 ? S1 Nb1 S1 67.67(8) 2_565 8_665 ? S1 Nb1 S1 125.19(8) . 8_665 ? F2 Nb2 F3 91.14(16) . 3 ? F2 Nb2 F3 91.14(16) . 4 ? F3 Nb2 F3 177.7(3) 3 4 ? F2 Nb2 F3 91.14(16) . . ? F3 Nb2 F3 89.977(7) 3 . ? F3 Nb2 F3 89.977(7) 4 . ? F2 Nb2 F3 91.14(16) . 2 ? F3 Nb2 F3 89.977(7) 3 2 ? F3 Nb2 F3 89.977(7) 4 2 ? F3 Nb2 F3 177.7(3) . 2 ? F2 Nb2 F4 180.000(1) . . ? F3 Nb2 F4 88.86(16) 3 . ? F3 Nb2 F4 88.86(16) 4 . ? F3 Nb2 F4 88.86(16) . . ? F3 Nb2 F4 88.86(16) 2 . ? C2 S1 C1 101.5(4) . . ? C2 S1 Nb1 105.5(3) . . ? C1 S1 Nb1 103.6(3) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.640 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.175 #===END OF CIF ============================================================== # 09mj08 data_09mj08 _database_code_depnum_ccdc_archive 'CCDC 723267' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-02-19 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrafluorobis[1,2-bis(methylthio)ethane-S,S']niobium(V) hexafluoroniobate(V) ; # S ligand name: # 2,5-dithiahexane # 1,2-bis(methylthio)ethane (I-Lab name) # 1,2-bis(methylsulfanyl)ethane (chemspider name) _chemical_name_common ;Tetrafluorobis(1,2-bis(methylthio)ethane-S,S')niobium(V) hexafluoroniobate(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 F4 Nb S4 1+, F6 Nb 1-' _chemical_formula_sum 'C8 H20 F10 Nb2 S4' _chemical_formula_structural '((C4 H10 S2)2 (Nb F4)) (Nb F6)' _chemical_formula_weight 620.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.0661(10) _cell_length_b 26.321(2) _cell_length_c 10.7327(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.252(5) _cell_angle_gamma 90.00 _cell_volume 3897.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19587 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 1.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8219 # 0.8234 shelxl _exptl_absorpt_correction_T_max 1.0000 # 0.9357 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23913 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8152 _reflns_number_gt 7749 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+25.1013P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 8152 _refine_ls_number_parameters 442 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.33718(3) 0.549514(17) 0.34651(4) 0.01682(10) Uani 1 1 d . . . Nb2 Nb 0.55422(3) 0.800108(17) 0.28475(5) 0.02159(11) Uani 1 1 d . . . Nb3 Nb 0.57910(4) 0.700887(17) 0.76601(5) 0.02197(11) Uani 1 1 d . . . Nb4 Nb 0.32985(3) 0.947150(17) 0.71113(5) 0.02116(11) Uani 1 1 d . . . S1 S 0.38361(10) 0.45361(5) 0.43071(13) 0.0224(3) Uani 1 1 d . . . S2 S 0.52475(10) 0.53672(6) 0.32618(15) 0.0265(3) Uani 1 1 d . . . S3 S 0.20526(10) 0.59103(5) 0.15424(13) 0.0225(3) Uani 1 1 d . . . S4 S 0.23126(9) 0.61347(5) 0.46200(13) 0.0230(3) Uani 1 1 d . . . S5 S 0.74828(10) 0.78483(5) 0.31684(15) 0.0268(3) Uani 1 1 d . . . S6 S 0.57749(12) 0.69787(6) 0.31746(17) 0.0344(3) Uani 1 1 d . . . S7 S 0.44709(9) 0.85532(5) 0.41814(13) 0.0216(3) Uani 1 1 d . . . S8 S 0.43790(10) 0.85973(5) 0.11166(13) 0.0261(3) Uani 1 1 d . . . F1 F 0.2229(2) 0.51456(11) 0.3702(3) 0.0229(7) Uani 1 1 d . . . F2 F 0.4011(2) 0.55667(11) 0.5179(3) 0.0213(6) Uani 1 1 d . . . F3 F 0.3879(2) 0.61335(12) 0.3052(3) 0.0256(7) Uani 1 1 d . . . F4 F 0.3379(2) 0.51465(11) 0.1929(3) 0.0227(6) Uani 1 1 d . . . F5 F 0.4308(2) 0.76715(12) 0.2411(3) 0.0295(8) Uani 1 1 d . . . F6 F 0.5845(2) 0.78291(14) 0.4597(4) 0.0360(9) Uani 1 1 d . . . F7 F 0.6188(2) 0.86377(11) 0.3119(3) 0.0236(7) Uani 1 1 d . . . F8 F 0.5841(3) 0.78713(17) 0.1250(4) 0.0416(10) Uani 1 1 d . . . F9 F 0.6471(3) 0.64068(15) 0.8135(6) 0.0574(13) Uani 1 1 d . . . F10 F 0.4834(3) 0.68044(15) 0.8561(4) 0.0421(10) Uani 1 1 d . . . F11 F 0.6471(3) 0.7307(2) 0.9142(5) 0.0702(16) Uani 1 1 d . . . F12 F 0.6799(3) 0.7223(2) 0.6852(5) 0.0608(14) Uani 1 1 d . . . F13 F 0.5158(4) 0.6703(3) 0.6185(6) 0.114(3) Uani 1 1 d . . . F14 F 0.5093(4) 0.76082(19) 0.7239(6) 0.0780(19) Uani 1 1 d . . . F15 F 0.4019(3) 0.88697(13) 0.7126(4) 0.0417(9) Uani 1 1 d . . . F16 F 0.2200(3) 0.91260(16) 0.6217(4) 0.0501(11) Uani 1 1 d . . . F17 F 0.2980(3) 0.92769(15) 0.8678(4) 0.0396(9) Uani 1 1 d . . . F18 F 0.4416(2) 0.98013(13) 0.8011(4) 0.0316(8) Uani 1 1 d . . . F19 F 0.3638(3) 0.96742(18) 0.5582(4) 0.0530(11) Uani 1 1 d . . . F20 F 0.2550(3) 1.00620(14) 0.7127(4) 0.0447(10) Uani 1 1 d . . . C1 C 0.3335(4) 0.4147(2) 0.2953(6) 0.0312(14) Uani 1 1 d . . . H1A H 0.3573 0.4268 0.2206 0.047 Uiso 1 1 calc R . . H1B H 0.2626 0.4169 0.2792 0.047 Uiso 1 1 calc R . . H1C H 0.3535 0.3794 0.3127 0.047 Uiso 1 1 calc R . . C2 C 0.5122(4) 0.4443(2) 0.4420(6) 0.0287(13) Uani 1 1 d . . . H2A H 0.5470 0.4578 0.5245 0.034 Uiso 1 1 calc R . . H2B H 0.5258 0.4075 0.4402 0.034 Uiso 1 1 calc R . . C3 C 0.5504(4) 0.4698(2) 0.3368(6) 0.0298(13) Uani 1 1 d . . . H3A H 0.5213 0.4535 0.2551 0.036 Uiso 1 1 calc R . . H3B H 0.6214 0.4648 0.3506 0.036 Uiso 1 1 calc R . . C4 C 0.5972(4) 0.5598(3) 0.4724(7) 0.0388(16) Uani 1 1 d . . . H4A H 0.5778 0.5427 0.5444 0.058 Uiso 1 1 calc R . . H4B H 0.5876 0.5965 0.4790 0.058 Uiso 1 1 calc R . . H4C H 0.6658 0.5529 0.4731 0.058 Uiso 1 1 calc R . . C5 C 0.1154(4) 0.5423(2) 0.1096(6) 0.0320(14) Uani 1 1 d . . . H5A H 0.0910 0.5312 0.1847 0.048 Uiso 1 1 calc R . . H5B H 0.1446 0.5133 0.0736 0.048 Uiso 1 1 calc R . . H5C H 0.0617 0.5558 0.0461 0.048 Uiso 1 1 calc R . . C6 C 0.1381(4) 0.6396(2) 0.2188(6) 0.0271(12) Uani 1 1 d . . . H6A H 0.1743 0.6721 0.2232 0.033 Uiso 1 1 calc R . . H6B H 0.0748 0.6447 0.1608 0.033 Uiso 1 1 calc R . . C7 C 0.1207(4) 0.6265(2) 0.3498(5) 0.0253(12) Uani 1 1 d . . . H7A H 0.0780 0.5964 0.3435 0.030 Uiso 1 1 calc R . . H7B H 0.0866 0.6551 0.3818 0.030 Uiso 1 1 calc R . . C8 C 0.2917(5) 0.6738(2) 0.4777(7) 0.0343(14) Uani 1 1 d . . . H8A H 0.2971 0.6864 0.3934 0.051 Uiso 1 1 calc R . . H8B H 0.3566 0.6700 0.5301 0.051 Uiso 1 1 calc R . . H8C H 0.2543 0.6981 0.5181 0.051 Uiso 1 1 calc R . . C9 C 0.7973(4) 0.7925(3) 0.4834(6) 0.0330(14) Uani 1 1 d . . . H9A H 0.7604 0.7716 0.5328 0.050 Uiso 1 1 calc R . . H9B H 0.7929 0.8283 0.5070 0.050 Uiso 1 1 calc R . . H9C H 0.8654 0.7818 0.5013 0.050 Uiso 1 1 calc R . . C10 C 0.7682(5) 0.7183(2) 0.2943(8) 0.0404(17) Uani 1 1 d . . . H10A H 0.7517 0.7102 0.2026 0.049 Uiso 1 1 calc R . . H10B H 0.8375 0.7103 0.3250 0.049 Uiso 1 1 calc R . . C11 C 0.7055(5) 0.6851(3) 0.3669(8) 0.0486(19) Uani 1 1 d . . . H11A H 0.7251 0.6917 0.4591 0.058 Uiso 1 1 calc R . . H11B H 0.7178 0.6488 0.3520 0.058 Uiso 1 1 calc R . . C12 C 0.5519(6) 0.6712(3) 0.1616(8) 0.0501(19) Uani 1 1 d . . . H12A H 0.5785 0.6933 0.1033 0.075 Uiso 1 1 calc R . . H12B H 0.4816 0.6683 0.1328 0.075 Uiso 1 1 calc R . . H12C H 0.5815 0.6375 0.1631 0.075 Uiso 1 1 calc R . . C13 C 0.3643(5) 0.8100(2) 0.4617(7) 0.0336(14) Uani 1 1 d . . . H13A H 0.3200 0.8272 0.5078 0.050 Uiso 1 1 calc R . . H13B H 0.4007 0.7838 0.5162 0.050 Uiso 1 1 calc R . . H13C H 0.3270 0.7941 0.3849 0.050 Uiso 1 1 calc R . . C14 C 0.3658(4) 0.8973(2) 0.3159(6) 0.0238(11) Uani 1 1 d . . . H14A H 0.3070 0.9025 0.3520 0.029 Uiso 1 1 calc R . . H14B H 0.3977 0.9308 0.3133 0.029 Uiso 1 1 calc R . . C15 C 0.3368(4) 0.8774(2) 0.1836(6) 0.0264(12) Uani 1 1 d . . . H15A H 0.2981 0.9037 0.1302 0.032 Uiso 1 1 calc R . . H15B H 0.2947 0.8473 0.1847 0.032 Uiso 1 1 calc R . . C16 C 0.4987(4) 0.9201(2) 0.1080(7) 0.0322(14) Uani 1 1 d . . . H16A H 0.4555 0.9439 0.0540 0.048 Uiso 1 1 calc R . . H16B H 0.5577 0.9152 0.0737 0.048 Uiso 1 1 calc R . . H16C H 0.5158 0.9338 0.1943 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0164(2) 0.0185(2) 0.0163(2) 0.00228(18) 0.00503(16) 0.00296(18) Nb2 0.0199(2) 0.0154(2) 0.0284(3) -0.0030(2) 0.00223(19) 0.00329(18) Nb3 0.0171(2) 0.0240(2) 0.0248(3) 0.0025(2) 0.00412(18) 0.0011(2) Nb4 0.0205(2) 0.0171(2) 0.0254(3) -0.00032(19) 0.00316(19) -0.00244(18) S1 0.0281(7) 0.0216(6) 0.0196(7) 0.0035(5) 0.0094(5) 0.0066(5) S2 0.0195(6) 0.0315(7) 0.0309(8) 0.0048(6) 0.0108(5) 0.0042(5) S3 0.0234(6) 0.0254(6) 0.0185(7) 0.0024(5) 0.0034(5) 0.0046(5) S4 0.0215(6) 0.0270(6) 0.0201(7) -0.0001(5) 0.0032(5) 0.0086(5) S5 0.0236(7) 0.0256(7) 0.0330(8) 0.0046(6) 0.0101(6) 0.0051(6) S6 0.0384(8) 0.0298(7) 0.0364(9) 0.0047(6) 0.0105(7) 0.0050(6) S7 0.0191(6) 0.0247(6) 0.0201(7) -0.0016(5) 0.0016(5) -0.0011(5) S8 0.0311(7) 0.0269(7) 0.0187(7) -0.0014(5) 0.0009(5) 0.0063(6) F1 0.0208(15) 0.0207(15) 0.0273(18) 0.0024(13) 0.0050(12) 0.0003(12) F2 0.0198(14) 0.0267(15) 0.0175(16) -0.0003(12) 0.0036(12) 0.0021(12) F3 0.0242(16) 0.0222(15) 0.0315(19) 0.0024(13) 0.0080(13) -0.0010(13) F4 0.0294(16) 0.0217(15) 0.0185(16) 0.0002(12) 0.0083(12) 0.0054(13) F5 0.0218(16) 0.0218(16) 0.043(2) -0.0077(14) 0.0011(14) -0.0018(13) F6 0.0233(17) 0.040(2) 0.046(2) 0.0197(18) 0.0083(15) 0.0066(15) F7 0.0231(15) 0.0170(14) 0.0309(18) 0.0011(13) 0.0059(13) -0.0002(12) F8 0.038(2) 0.056(3) 0.030(2) -0.0130(18) 0.0070(16) 0.0142(18) F9 0.043(2) 0.0277(19) 0.113(4) 0.024(2) 0.043(2) 0.0127(18) F10 0.0283(19) 0.038(2) 0.065(3) 0.0118(19) 0.0223(18) 0.0027(16) F11 0.037(2) 0.097(4) 0.077(4) -0.054(3) 0.012(2) -0.012(2) F12 0.041(2) 0.080(3) 0.070(3) 0.047(3) 0.031(2) 0.024(2) F13 0.041(3) 0.208(8) 0.086(5) -0.094(5) -0.004(3) 0.001(4) F14 0.060(3) 0.062(3) 0.125(5) 0.062(3) 0.049(3) 0.042(3) F15 0.043(2) 0.0265(18) 0.057(3) -0.0123(18) 0.0130(19) 0.0048(16) F16 0.037(2) 0.047(2) 0.059(3) -0.006(2) -0.0074(19) -0.0183(19) F17 0.043(2) 0.043(2) 0.038(2) 0.0056(18) 0.0206(17) -0.0030(18) F18 0.0229(16) 0.0294(17) 0.041(2) -0.0045(15) 0.0024(14) -0.0047(14) F19 0.068(3) 0.057(3) 0.036(2) 0.013(2) 0.013(2) -0.016(2) F20 0.035(2) 0.0283(19) 0.065(3) 0.0008(18) -0.0029(18) 0.0067(16) C1 0.033(3) 0.015(2) 0.045(4) -0.002(2) 0.006(3) -0.001(2) C2 0.027(3) 0.028(3) 0.029(3) 0.000(2) 0.002(2) 0.008(2) C3 0.025(3) 0.025(3) 0.040(4) -0.006(3) 0.009(2) 0.005(2) C4 0.020(3) 0.044(4) 0.051(4) -0.006(3) 0.003(3) -0.009(3) C5 0.029(3) 0.032(3) 0.031(4) -0.006(3) -0.005(3) 0.004(2) C6 0.025(3) 0.031(3) 0.025(3) 0.002(2) 0.005(2) 0.011(2) C7 0.020(2) 0.030(3) 0.024(3) 0.006(2) 0.000(2) 0.008(2) C8 0.033(3) 0.026(3) 0.043(4) -0.008(3) 0.005(3) 0.003(2) C9 0.023(3) 0.043(4) 0.032(4) 0.005(3) 0.004(2) 0.000(3) C10 0.032(3) 0.032(3) 0.058(5) 0.000(3) 0.013(3) 0.017(3) C11 0.040(4) 0.042(4) 0.061(5) 0.008(4) 0.004(3) 0.013(3) C12 0.065(5) 0.034(4) 0.051(5) -0.011(3) 0.009(4) 0.005(3) C13 0.032(3) 0.033(3) 0.037(4) 0.005(3) 0.010(3) -0.007(3) C14 0.025(3) 0.020(2) 0.027(3) 0.002(2) 0.006(2) 0.004(2) C15 0.018(2) 0.027(3) 0.034(3) 0.009(2) 0.003(2) 0.004(2) C16 0.030(3) 0.030(3) 0.037(4) 0.009(3) 0.009(3) 0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 F4 1.889(3) . ? Nb1 F2 1.893(3) . ? Nb1 F3 1.911(3) . ? Nb1 F1 1.912(3) . ? Nb1 S4 2.7039(14) . ? Nb1 S2 2.7105(14) . ? Nb1 S1 2.7176(13) . ? Nb1 S3 2.7205(14) . ? Nb2 F8 1.875(4) . ? Nb2 F6 1.897(4) . ? Nb2 F7 1.901(3) . ? Nb2 F5 1.916(3) . ? Nb2 S7 2.6970(15) . ? Nb2 S5 2.7138(15) . ? Nb2 S8 2.7212(14) . ? Nb2 S6 2.7252(16) . ? Nb3 F13 1.843(5) . ? Nb3 F11 1.861(5) . ? Nb3 F14 1.866(4) . ? Nb3 F9 1.870(4) . ? Nb3 F10 1.883(4) . ? Nb3 F12 1.887(4) . ? Nb4 F19 1.875(4) . ? Nb4 F20 1.879(4) . ? Nb4 F15 1.879(4) . ? Nb4 F16 1.886(4) . ? Nb4 F18 1.889(3) . ? Nb4 F17 1.893(4) . ? S1 C1 1.804(6) . ? S1 C2 1.806(6) . ? S2 C3 1.796(6) . ? S2 C4 1.802(7) . ? S3 C5 1.798(6) . ? S3 C6 1.807(6) . ? S4 C8 1.794(6) . ? S4 C7 1.804(5) . ? S5 C10 1.797(6) . ? S5 C9 1.798(7) . ? S6 C12 1.785(8) . ? S6 C11 1.806(7) . ? S7 C13 1.792(6) . ? S7 C14 1.801(5) . ? S8 C15 1.806(6) . ? S8 C16 1.807(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.500(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.514(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.554(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.494(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F4 Nb1 F2 144.54(13) . . ? F4 Nb1 F3 99.13(14) . . ? F2 Nb1 F3 90.60(14) . . ? F4 Nb1 F1 91.71(14) . . ? F2 Nb1 F1 99.84(14) . . ? F3 Nb1 F1 144.63(13) . . ? F4 Nb1 S4 143.12(10) . . ? F2 Nb1 S4 72.06(10) . . ? F3 Nb1 S4 79.80(10) . . ? F1 Nb1 S4 71.69(10) . . ? F4 Nb1 S2 72.45(10) . . ? F2 Nb1 S2 78.80(10) . . ? F3 Nb1 S2 71.18(10) . . ? F1 Nb1 S2 143.89(10) . . ? S4 Nb1 S2 138.27(5) . . ? F4 Nb1 S1 78.29(10) . . ? F2 Nb1 S1 74.42(10) . . ? F3 Nb1 S1 144.85(10) . . ? F1 Nb1 S1 70.28(9) . . ? S4 Nb1 S1 122.96(5) . . ? S2 Nb1 S1 74.74(4) . . ? F4 Nb1 S3 69.63(10) . . ? F2 Nb1 S3 145.24(10) . . ? F3 Nb1 S3 72.59(10) . . ? F1 Nb1 S3 80.05(10) . . ? S4 Nb1 S3 75.07(4) . . ? S2 Nb1 S3 121.29(5) . . ? S1 Nb1 S3 135.19(5) . . ? F8 Nb2 F6 144.54(17) . . ? F8 Nb2 F7 96.58(18) . . ? F6 Nb2 F7 92.90(16) . . ? F8 Nb2 F5 92.77(18) . . ? F6 Nb2 F5 98.72(16) . . ? F7 Nb2 F5 145.08(13) . . ? F8 Nb2 S7 146.30(13) . . ? F6 Nb2 S7 69.14(12) . . ? F7 Nb2 S7 75.16(10) . . ? F5 Nb2 S7 78.47(11) . . ? F8 Nb2 S5 71.90(12) . . ? F6 Nb2 S5 79.23(11) . . ? F7 Nb2 S5 70.86(10) . . ? F5 Nb2 S5 143.64(11) . . ? S7 Nb2 S5 131.67(5) . . ? F8 Nb2 S8 72.12(13) . . ? F6 Nb2 S8 143.33(12) . . ? F7 Nb2 S8 78.58(10) . . ? F5 Nb2 S8 72.46(11) . . ? S7 Nb2 S8 74.21(4) . . ? S5 Nb2 S8 128.90(5) . . ? F8 Nb2 S6 83.98(14) . . ? F6 Nb2 S6 68.83(13) . . ? F7 Nb2 S6 143.96(10) . . ? F5 Nb2 S6 70.41(10) . . ? S7 Nb2 S6 121.95(5) . . ? S5 Nb2 S6 75.21(5) . . ? S8 Nb2 S6 134.31(5) . . ? F13 Nb3 F11 178.0(2) . . ? F13 Nb3 F14 91.1(3) . . ? F11 Nb3 F14 90.5(3) . . ? F13 Nb3 F9 90.0(3) . . ? F11 Nb3 F9 88.5(3) . . ? F14 Nb3 F9 177.9(2) . . ? F13 Nb3 F10 92.4(3) . . ? F11 Nb3 F10 88.9(2) . . ? F14 Nb3 F10 88.34(19) . . ? F9 Nb3 F10 89.84(17) . . ? F13 Nb3 F12 90.9(3) . . ? F11 Nb3 F12 87.7(2) . . ? F14 Nb3 F12 92.5(2) . . ? F9 Nb3 F12 89.28(18) . . ? F10 Nb3 F12 176.5(2) . . ? F19 Nb4 F20 90.6(2) . . ? F19 Nb4 F15 91.0(2) . . ? F20 Nb4 F15 178.1(2) . . ? F19 Nb4 F16 90.9(2) . . ? F20 Nb4 F16 89.92(18) . . ? F15 Nb4 F16 89.13(18) . . ? F19 Nb4 F18 89.31(18) . . ? F20 Nb4 F18 91.56(16) . . ? F15 Nb4 F18 89.38(16) . . ? F16 Nb4 F18 178.50(18) . . ? F19 Nb4 F17 178.6(2) . . ? F20 Nb4 F17 89.20(19) . . ? F15 Nb4 F17 89.16(19) . . ? F16 Nb4 F17 90.5(2) . . ? F18 Nb4 F17 89.29(17) . . ? C1 S1 C2 101.9(3) . . ? C1 S1 Nb1 103.2(2) . . ? C2 S1 Nb1 108.7(2) . . ? C3 S2 C4 101.7(3) . . ? C3 S2 Nb1 107.7(2) . . ? C4 S2 Nb1 106.4(2) . . ? C5 S3 C6 102.4(3) . . ? C5 S3 Nb1 104.8(2) . . ? C6 S3 Nb1 108.91(19) . . ? C8 S4 C7 103.0(3) . . ? C8 S4 Nb1 107.5(2) . . ? C7 S4 Nb1 107.0(2) . . ? C10 S5 C9 101.8(3) . . ? C10 S5 Nb2 107.8(2) . . ? C9 S5 Nb2 106.9(2) . . ? C12 S6 C11 102.1(4) . . ? C12 S6 Nb2 105.7(3) . . ? C11 S6 Nb2 108.0(3) . . ? C13 S7 C14 101.6(3) . . ? C13 S7 Nb2 103.8(2) . . ? C14 S7 Nb2 111.2(2) . . ? C15 S8 C16 101.4(3) . . ? C15 S8 Nb2 105.99(19) . . ? C16 S8 Nb2 107.3(2) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 112.9(4) . . ? C3 C2 H2A 109.0 . . ? S1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? S1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 S2 112.9(4) . . ? C2 C3 H3A 109.0 . . ? S2 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? S2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S3 C5 H5A 109.5 . . ? S3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 S3 112.7(4) . . ? C7 C6 H6A 109.1 . . ? S3 C6 H6A 109.1 . . ? C7 C6 H6B 109.1 . . ? S3 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 C7 S4 112.9(4) . . ? C6 C7 H7A 109.0 . . ? S4 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? S4 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? S4 C8 H8A 109.5 . . ? S4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S5 C9 H9A 109.5 . . ? S5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 S5 111.2(5) . . ? C11 C10 H10A 109.4 . . ? S5 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? S5 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 S6 112.2(5) . . ? C10 C11 H11A 109.2 . . ? S6 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? S6 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? S6 C12 H12A 109.5 . . ? S6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S7 C13 H13A 109.5 . . ? S7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? S7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 S7 112.8(4) . . ? C15 C14 H14A 109.0 . . ? S7 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? S7 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 S8 113.9(4) . . ? C14 C15 H15A 108.8 . . ? S8 C15 H15A 108.8 . . ? C14 C15 H15B 108.8 . . ? S8 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? S8 C16 H16A 109.5 . . ? S8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.019 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.121 #===END OF CIF ============================================================== # 09mj07 data_09mj07 _database_code_depnum_ccdc_archive 'CCDC 723268' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2009-02-17 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrafluorobis(1,2-bis(isopropylthio)ethane-S,S')niobium(V) hexafluoroniobate(V) ; # S ligand name: # 1,2-bis(isopropylthio)ethane # 2-{[2-(isopropylthio)ethyl]thio}propane (i-Lab IUPAC name) # 2,7-dimethyl-3,6-dithiaoctane # 2-(2-isopropylsulfanylethylsulfanyl)propane (from chemspider) _chemical_name_common ;Tetrafluorobis(1,2-bis(isopropylthio)ethane-S,S')niobium(V) hexafluoroniobate(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 F4 Nb S4 1+, F6 Nb1 1-' _chemical_formula_sum 'C16 H36 F10 Nb2 S4' _chemical_formula_structural '((C8 H18 S2)2 (F4 Nb)) (F6 Nb)' _chemical_formula_weight 732.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2850(10) _cell_length_b 11.6895(15) _cell_length_c 13.5404(15) _cell_angle_alpha 115.206(7) _cell_angle_beta 90.596(10) _cell_angle_gamma 110.136(10) _cell_volume 1359.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 49250 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7638 # 0.7920 shelxl _exptl_absorpt_correction_T_max 1.0000 # 0.9527 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27957 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.71 _reflns_number_total 6180 _reflns_number_gt 5146 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+5.7487P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6180 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.86971(4) 0.59002(4) 0.31573(3) 0.01678(10) Uani 1 1 d . . . Nb2 Nb 0.0000 0.0000 0.0000 0.03102(16) Uani 1 2 d S . . Nb3 Nb 0.5000 1.0000 0.5000 0.02636(14) Uani 1 2 d S . . F1 F 1.0161(2) 0.5263(2) 0.3191(2) 0.0210(5) Uani 1 1 d . . . F2 F 0.6769(2) 0.5555(2) 0.3273(2) 0.0199(5) Uani 1 1 d . . . F3 F 0.8251(2) 0.5265(2) 0.16043(19) 0.0205(5) Uani 1 1 d . . . F4 F 0.9589(3) 0.7489(2) 0.45523(19) 0.0219(5) Uani 1 1 d . . . F5 F -0.0811(4) -0.1684(3) 0.0049(3) 0.0495(8) Uani 1 1 d . . . F6 F 0.1802(4) -0.0018(4) 0.0188(4) 0.0662(11) Uani 1 1 d . . . F7 F 0.0168(4) 0.0932(4) 0.1556(3) 0.0594(10) Uani 1 1 d . . . F8 F 0.4501(3) 0.8253(3) 0.3785(3) 0.0441(8) Uani 1 1 d . . . F9 F 0.4029(4) 1.0498(4) 0.4164(3) 0.0550(9) Uani 1 1 d . . . F10 F 0.6651(4) 1.0651(3) 0.4484(3) 0.0486(8) Uani 1 1 d . . . S1 S 0.84225(10) 0.52194(10) 0.48698(8) 0.0189(2) Uani 1 1 d . . . S2 S 0.75756(11) 0.30985(11) 0.21831(9) 0.0209(2) Uani 1 1 d . . . S3 S 0.81235(11) 0.80072(11) 0.31967(9) 0.0212(2) Uani 1 1 d . . . S4 S 1.10712(11) 0.74737(11) 0.27437(9) 0.0232(2) Uani 1 1 d . . . C1 C 0.6779(5) 0.5189(6) 0.6453(4) 0.0325(11) Uani 1 1 d . . . H1A H 0.7636 0.5733 0.7024 0.049 Uiso 1 1 calc R . . H1B H 0.6608 0.4214 0.6151 0.049 Uiso 1 1 calc R . . H1C H 0.5976 0.5353 0.6782 0.049 Uiso 1 1 calc R . . C2 C 0.7270(5) 0.7120(5) 0.5943(4) 0.0278(10) Uani 1 1 d . . . H2A H 0.6478 0.7322 0.6264 0.042 Uiso 1 1 calc R . . H2B H 0.7404 0.7350 0.5326 0.042 Uiso 1 1 calc R . . H2C H 0.8128 0.7664 0.6513 0.042 Uiso 1 1 calc R . . C3 C 0.6960(4) 0.5605(5) 0.5521(4) 0.0222(9) Uani 1 1 d . . . H3 H 0.6074 0.5059 0.4950 0.027 Uiso 1 1 calc R . . C4 C 0.7743(5) 0.3367(4) 0.4328(4) 0.0233(9) Uani 1 1 d . . . H4A H 0.8118 0.3135 0.4862 0.028 Uiso 1 1 calc R . . H4B H 0.6703 0.3006 0.4239 0.028 Uiso 1 1 calc R . . C5 C 0.8159(5) 0.2702(4) 0.3217(4) 0.0234(9) Uani 1 1 d . . . H5A H 0.7757 0.1696 0.2938 0.028 Uiso 1 1 calc R . . H5B H 0.9198 0.3007 0.3326 0.028 Uiso 1 1 calc R . . C6 C 0.5658(4) 0.2481(4) 0.2078(4) 0.0226(9) Uani 1 1 d . . . H6 H 0.5423 0.3076 0.2778 0.027 Uiso 1 1 calc R . . C7 C 0.5063(5) 0.2604(5) 0.1111(4) 0.0290(10) Uani 1 1 d . . . H7A H 0.5286 0.2017 0.0422 0.043 Uiso 1 1 calc R . . H7B H 0.5482 0.3558 0.1241 0.043 Uiso 1 1 calc R . . H7C H 0.4039 0.2317 0.1045 0.043 Uiso 1 1 calc R . . C8 C 0.5050(5) 0.1001(5) 0.1896(4) 0.0315(10) Uani 1 1 d . . . H8A H 0.4019 0.0643 0.1716 0.047 Uiso 1 1 calc R . . H8B H 0.5336 0.0970 0.2574 0.047 Uiso 1 1 calc R . . H8C H 0.5404 0.0441 0.1281 0.047 Uiso 1 1 calc R . . C9 C 0.7095(6) 0.8841(5) 0.1854(4) 0.0353(11) Uani 1 1 d . . . H9A H 0.6624 0.8613 0.1123 0.053 Uiso 1 1 calc R . . H9B H 0.8034 0.9562 0.2042 0.053 Uiso 1 1 calc R . . H9C H 0.6538 0.9166 0.2414 0.053 Uiso 1 1 calc R . . C10 C 0.5779(5) 0.6446(5) 0.1577(4) 0.0334(11) Uani 1 1 d . . . H10A H 0.5270 0.6758 0.2180 0.050 Uiso 1 1 calc R . . H10B H 0.5885 0.5617 0.1514 0.050 Uiso 1 1 calc R . . H10C H 0.5250 0.6243 0.0877 0.050 Uiso 1 1 calc R . . C11 C 0.7231(5) 0.7565(5) 0.1827(4) 0.0256(9) Uani 1 1 d . . . H11 H 0.7787 0.7222 0.1249 0.031 Uiso 1 1 calc R . . C12 C 0.9827(5) 0.9321(5) 0.3397(4) 0.0312(10) Uani 1 1 d . . . H12A H 0.9682 1.0084 0.3334 0.037 Uiso 1 1 calc R . . H12B H 1.0340 0.9688 0.4158 0.037 Uiso 1 1 calc R . . C13 C 1.0713(5) 0.8813(5) 0.2578(4) 0.0308(10) Uani 1 1 d . . . H13A H 1.1611 0.9578 0.2704 0.037 Uiso 1 1 calc R . . H13B H 1.0211 0.8442 0.1813 0.037 Uiso 1 1 calc R . . C14 C 1.1306(5) 0.6510(5) 0.1323(4) 0.0265(9) Uani 1 1 d . . . H14 H 1.0415 0.6156 0.0793 0.032 Uiso 1 1 calc R . . C15 C 1.2496(6) 0.7460(5) 0.1038(4) 0.0344(11) Uani 1 1 d . . . H15A H 1.3356 0.7861 0.1588 0.052 Uiso 1 1 calc R . . H15B H 1.2235 0.8192 0.1042 0.052 Uiso 1 1 calc R . . H15C H 1.2665 0.6937 0.0299 0.052 Uiso 1 1 calc R . . C16 C 1.1628(5) 0.5310(5) 0.1258(4) 0.0312(10) Uani 1 1 d . . . H16A H 1.1853 0.4844 0.0528 0.047 Uiso 1 1 calc R . . H16B H 1.0804 0.4667 0.1365 0.047 Uiso 1 1 calc R . . H16C H 1.2434 0.5645 0.1839 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.01604(18) 0.01686(18) 0.01776(18) 0.00907(14) 0.00334(13) 0.00521(14) Nb2 0.0295(3) 0.0328(3) 0.0276(3) 0.0196(3) -0.0012(2) 0.0012(3) Nb3 0.0348(3) 0.0207(3) 0.0230(3) 0.0118(2) 0.0056(2) 0.0078(2) F1 0.0167(11) 0.0248(12) 0.0261(12) 0.0157(11) 0.0065(9) 0.0078(10) F2 0.0147(11) 0.0227(12) 0.0246(12) 0.0127(10) 0.0037(9) 0.0073(9) F3 0.0207(12) 0.0211(12) 0.0180(11) 0.0098(10) 0.0045(9) 0.0050(10) F4 0.0229(12) 0.0196(12) 0.0206(12) 0.0094(10) 0.0029(9) 0.0050(10) F5 0.065(2) 0.0366(17) 0.0460(19) 0.0273(15) 0.0141(16) 0.0071(16) F6 0.039(2) 0.072(3) 0.090(3) 0.042(2) -0.0018(19) 0.0167(19) F7 0.075(3) 0.051(2) 0.0283(16) 0.0181(16) 0.0040(16) -0.0019(19) F8 0.0449(18) 0.0280(15) 0.0400(17) 0.0028(14) 0.0051(14) 0.0088(14) F9 0.073(3) 0.054(2) 0.050(2) 0.0317(18) -0.0010(18) 0.0290(19) F10 0.053(2) 0.0349(17) 0.052(2) 0.0202(15) 0.0264(16) 0.0098(15) S1 0.0178(5) 0.0206(5) 0.0209(5) 0.0119(4) 0.0045(4) 0.0071(4) S2 0.0218(5) 0.0197(5) 0.0220(5) 0.0102(4) 0.0056(4) 0.0080(4) S3 0.0249(5) 0.0196(5) 0.0216(5) 0.0109(4) 0.0058(4) 0.0095(4) S4 0.0210(5) 0.0206(5) 0.0257(5) 0.0108(4) 0.0059(4) 0.0053(4) C1 0.032(3) 0.044(3) 0.037(3) 0.030(2) 0.020(2) 0.018(2) C2 0.028(2) 0.031(2) 0.033(2) 0.018(2) 0.0148(19) 0.0149(19) C3 0.019(2) 0.030(2) 0.026(2) 0.0176(19) 0.0073(16) 0.0126(17) C4 0.024(2) 0.018(2) 0.028(2) 0.0148(18) 0.0000(17) 0.0043(17) C5 0.025(2) 0.022(2) 0.028(2) 0.0131(18) 0.0056(17) 0.0120(17) C6 0.018(2) 0.019(2) 0.025(2) 0.0094(17) 0.0028(16) 0.0018(16) C7 0.029(2) 0.029(2) 0.027(2) 0.015(2) 0.0004(18) 0.0061(19) C8 0.031(2) 0.023(2) 0.039(3) 0.017(2) 0.000(2) 0.0041(19) C9 0.051(3) 0.035(3) 0.030(2) 0.017(2) 0.008(2) 0.025(2) C10 0.034(3) 0.029(2) 0.036(3) 0.015(2) -0.002(2) 0.012(2) C11 0.033(2) 0.026(2) 0.021(2) 0.0095(18) 0.0041(18) 0.0163(19) C12 0.035(3) 0.019(2) 0.037(3) 0.013(2) 0.007(2) 0.0087(19) C13 0.031(2) 0.027(2) 0.039(3) 0.020(2) 0.009(2) 0.0087(19) C14 0.025(2) 0.032(2) 0.021(2) 0.0135(19) 0.0074(17) 0.0075(19) C15 0.035(3) 0.037(3) 0.034(3) 0.021(2) 0.014(2) 0.010(2) C16 0.035(3) 0.030(2) 0.027(2) 0.011(2) 0.0092(19) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 F3 1.897(2) . ? Nb1 F1 1.904(2) . ? Nb1 F2 1.905(2) . ? Nb1 F4 1.913(2) . ? Nb1 S3 2.7030(11) . ? Nb1 S4 2.7336(12) . ? Nb1 S2 2.7357(12) . ? Nb1 S1 2.7424(11) . ? Nb2 F6 1.877(4) . ? Nb2 F6 1.877(4) 2 ? Nb2 F5 1.886(3) 2 ? Nb2 F5 1.886(3) . ? Nb2 F7 1.888(3) 2 ? Nb2 F7 1.888(3) . ? Nb3 F8 1.881(3) 2_676 ? Nb3 F8 1.881(3) . ? Nb3 F10 1.881(3) . ? Nb3 F10 1.881(3) 2_676 ? Nb3 F9 1.885(3) 2_676 ? Nb3 F9 1.885(3) . ? S1 C4 1.819(4) . ? S1 C3 1.843(4) . ? S2 C5 1.807(4) . ? S2 C6 1.832(4) . ? S3 C12 1.812(5) . ? S3 C11 1.836(4) . ? S4 C13 1.825(5) . ? S4 C14 1.838(5) . ? C1 C3 1.526(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.519(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3 1.0000 . ? C4 C5 1.515(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.521(6) . ? C6 C8 1.527(6) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.531(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.524(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 1.0000 . ? C12 C13 1.499(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(7) . ? C14 C16 1.515(7) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Nb1 F1 99.35(10) . . ? F3 Nb1 F2 90.69(10) . . ? F1 Nb1 F2 143.70(10) . . ? F3 Nb1 F4 144.48(10) . . ? F1 Nb1 F4 91.73(11) . . ? F2 Nb1 F4 100.10(11) . . ? F3 Nb1 S3 81.26(8) . . ? F1 Nb1 S3 144.32(8) . . ? F2 Nb1 S3 71.52(8) . . ? F4 Nb1 S3 70.57(8) . . ? F3 Nb1 S4 77.45(8) . . ? F1 Nb1 S4 70.37(8) . . ? F2 Nb1 S4 145.87(8) . . ? F4 Nb1 S4 74.75(8) . . ? S3 Nb1 S4 75.07(4) . . ? F3 Nb1 S2 72.74(8) . . ? F1 Nb1 S2 70.83(8) . . ? F2 Nb1 S2 79.25(8) . . ? F4 Nb1 S2 142.39(8) . . ? S3 Nb1 S2 140.34(4) . . ? S4 Nb1 S2 125.47(4) . . ? F3 Nb1 S1 146.30(8) . . ? F1 Nb1 S1 75.26(8) . . ? F2 Nb1 S1 77.18(8) . . ? F4 Nb1 S1 69.18(8) . . ? S3 Nb1 S1 122.58(3) . . ? S4 Nb1 S1 128.54(3) . . ? S2 Nb1 S1 74.14(3) . . ? F6 Nb2 F6 180.0(3) . 2 ? F6 Nb2 F5 89.66(18) . 2 ? F6 Nb2 F5 90.34(18) 2 2 ? F6 Nb2 F5 90.34(18) . . ? F6 Nb2 F5 89.66(18) 2 . ? F5 Nb2 F5 180.0(3) 2 . ? F6 Nb2 F7 90.0(2) . 2 ? F6 Nb2 F7 90.0(2) 2 2 ? F5 Nb2 F7 89.44(15) 2 2 ? F5 Nb2 F7 90.56(15) . 2 ? F6 Nb2 F7 90.0(2) . . ? F6 Nb2 F7 90.0(2) 2 . ? F5 Nb2 F7 90.56(15) 2 . ? F5 Nb2 F7 89.44(15) . . ? F7 Nb2 F7 180.0(2) 2 . ? F8 Nb3 F8 180.00(17) 2_676 . ? F8 Nb3 F10 90.06(15) 2_676 . ? F8 Nb3 F10 89.94(15) . . ? F8 Nb3 F10 89.94(15) 2_676 2_676 ? F8 Nb3 F10 90.06(15) . 2_676 ? F10 Nb3 F10 180.000(1) . 2_676 ? F8 Nb3 F9 90.20(16) 2_676 2_676 ? F8 Nb3 F9 89.80(16) . 2_676 ? F10 Nb3 F9 90.23(18) . 2_676 ? F10 Nb3 F9 89.77(18) 2_676 2_676 ? F8 Nb3 F9 89.80(16) 2_676 . ? F8 Nb3 F9 90.20(16) . . ? F10 Nb3 F9 89.77(18) . . ? F10 Nb3 F9 90.23(18) 2_676 . ? F9 Nb3 F9 180.000(1) 2_676 . ? C4 S1 C3 100.9(2) . . ? C4 S1 Nb1 110.17(15) . . ? C3 S1 Nb1 108.85(14) . . ? C5 S2 C6 103.7(2) . . ? C5 S2 Nb1 103.93(15) . . ? C6 S2 Nb1 109.63(14) . . ? C12 S3 C11 103.9(2) . . ? C12 S3 Nb1 105.06(16) . . ? C11 S3 Nb1 111.14(15) . . ? C13 S4 C14 99.0(2) . . ? C13 S4 Nb1 108.40(16) . . ? C14 S4 Nb1 109.48(15) . . ? C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C1 112.0(4) . . ? C2 C3 S1 109.2(3) . . ? C1 C3 S1 108.9(3) . . ? C2 C3 H3 108.9 . . ? C1 C3 H3 108.9 . . ? S1 C3 H3 108.9 . . ? C5 C4 S1 110.9(3) . . ? C5 C4 H4A 109.5 . . ? S1 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? S1 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C4 C5 S2 113.4(3) . . ? C4 C5 H5A 108.9 . . ? S2 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? S2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C8 111.1(4) . . ? C7 C6 S2 107.0(3) . . ? C8 C6 S2 111.0(3) . . ? C7 C6 H6 109.3 . . ? C8 C6 H6 109.3 . . ? S2 C6 H6 109.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C10 C11 C9 110.5(4) . . ? C10 C11 S3 107.8(3) . . ? C9 C11 S3 109.1(3) . . ? C10 C11 H11 109.8 . . ? C9 C11 H11 109.8 . . ? S3 C11 H11 109.8 . . ? C13 C12 S3 113.2(3) . . ? C13 C12 H12A 108.9 . . ? S3 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? S3 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 S4 109.3(3) . . ? C12 C13 H13A 109.8 . . ? S4 C13 H13A 109.8 . . ? C12 C13 H13B 109.8 . . ? S4 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C16 111.3(4) . . ? C15 C14 S4 109.2(3) . . ? C16 C14 S4 108.7(3) . . ? C15 C14 H14 109.2 . . ? C16 C14 H14 109.2 . . ? S4 C14 H14 109.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C4 C5 S2 -57.3(4) . . . . ? S3 C12 C13 S4 -61.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.902 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.136 #===END OF CIF ============================================================== # 08mj33 data_08mj33 _database_code_depnum_ccdc_archive 'CCDC 723269' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-30 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Pentabromo(dimethylsulfide-S)niobium(V) ; _chemical_name_common Pentabromo(dimethylsulfide-S)niobium(V) _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Br5 Nb S' _chemical_formula_sum 'C2 H6 Br5 Nb S' _chemical_formula_weight 554.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2922(5) _cell_length_b 23.641(3) _cell_length_c 12.9072(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.267(5) _cell_angle_gamma 90.00 _cell_volume 2223.4(4) # shelx gave (3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23847 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 19.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5374 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24010 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5097 _reflns_number_gt 4222 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+20.1048P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5097 _refine_ls_number_parameters 175 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.97030(6) 1.06387(2) 0.23874(4) 0.01549(11) Uani 1 1 d . . . Nb2 Nb 0.53283(7) 0.80920(2) 0.20884(4) 0.01972(12) Uani 1 1 d . . . Br1 Br 0.68137(7) 1.06135(3) 0.13989(4) 0.02312(13) Uani 1 1 d . . . Br2 Br 0.84616(8) 1.09557(3) 0.40794(4) 0.02485(13) Uani 1 1 d . . . Br3 Br 1.04686(8) 1.16403(2) 0.20464(5) 0.02468(13) Uani 1 1 d . . . Br4 Br 1.16479(8) 1.03043(3) 0.09805(4) 0.02201(13) Uani 1 1 d . . . Br5 Br 0.95607(8) 0.96628(2) 0.30908(5) 0.02268(13) Uani 1 1 d . . . Br6 Br 0.81272(7) 0.81478(2) 0.31696(4) 0.02032(12) Uani 1 1 d . A . Br7 Br 0.55965(10) 0.90511(3) 0.13152(5) 0.03047(15) Uani 1 1 d . A . Br8 Br 0.32606(8) 0.84868(3) 0.34006(5) 0.02921(15) Uani 1 1 d . A . Br9 Br 0.45021(9) 0.71178(3) 0.25697(6) 0.03214(15) Uani 1 1 d . A . Br10 Br 0.66363(11) 0.77029(3) 0.04873(5) 0.03686(17) Uani 1 1 d . A . S1 S 1.31180(18) 1.07181(6) 0.32779(10) 0.0174(3) Uani 1 1 d . . . S2A S 0.1842(3) 0.79701(10) 0.13047(17) 0.0182(6) Uani 0.605(5) 1 d PD A 1 S2B S 0.2703(5) 0.81696(15) 0.0538(3) 0.0183(10) Uani 0.395(5) 1 d PD A 2 C1 C 1.3061(9) 1.1041(3) 0.4536(5) 0.0313(15) Uani 1 1 d . . . H1A H 1.2199 1.0835 0.4962 0.047 Uiso 1 1 calc R . . H1B H 1.2662 1.1435 0.4462 0.047 Uiso 1 1 calc R . . H1C H 1.4290 1.1029 0.4872 0.047 Uiso 1 1 calc R . . C2 C 1.3998(8) 1.0031(3) 0.3610(5) 0.0264(13) Uani 1 1 d . . . H2A H 1.5282 1.0065 0.3857 0.040 Uiso 1 1 calc R . . H2B H 1.3921 0.9787 0.2998 0.040 Uiso 1 1 calc R . . H2C H 1.3273 0.9867 0.4159 0.040 Uiso 1 1 calc R . . C3A C 0.0956(8) 0.8646(3) 0.0883(5) 0.0252(13) Uani 0.605(5) 1 d P A 1 H3A1 H 0.0974 0.8909 0.1471 0.038 Uiso 0.605(5) 1 calc PR A 1 H3A2 H -0.0308 0.8601 0.0609 0.038 Uiso 0.605(5) 1 calc PR A 1 H3A3 H 0.1718 0.8798 0.0339 0.038 Uiso 0.605(5) 1 calc PR A 1 C4A C 0.1732(12) 0.7545(3) 0.0214(7) 0.066(3) Uani 0.605(5) 1 d PD A 1 H4A1 H 0.2201 0.7167 0.0394 0.098 Uiso 0.605(5) 1 calc PR A 1 H4A2 H 0.2478 0.7711 -0.0323 0.098 Uiso 0.605(5) 1 calc PR A 1 H4A3 H 0.0455 0.7515 -0.0045 0.098 Uiso 0.605(5) 1 calc PR A 1 C3B C 0.0956(8) 0.8646(3) 0.0883(5) 0.0252(13) Uani 0.395(5) 1 d P A 2 H3B1 H 0.1505 0.9012 0.1076 0.038 Uiso 0.395(5) 1 calc PR A 2 H3B2 H 0.0308 0.8493 0.1472 0.038 Uiso 0.395(5) 1 calc PR A 2 H3B3 H 0.0087 0.8698 0.0292 0.038 Uiso 0.395(5) 1 calc PR A 2 C4B C 0.1732(12) 0.7545(3) 0.0214(7) 0.066(3) Uani 0.395(5) 1 d PD A 2 H4B1 H 0.2687 0.7277 0.0023 0.098 Uiso 0.395(5) 1 calc PR A 2 H4B2 H 0.0860 0.7598 -0.0375 0.098 Uiso 0.395(5) 1 calc PR A 2 H4B3 H 0.1084 0.7395 0.0807 0.098 Uiso 0.395(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0158(2) 0.0138(2) 0.0169(2) 0.00039(19) 0.00106(18) -0.00050(19) Nb2 0.0195(2) 0.0148(3) 0.0245(3) -0.0041(2) -0.0036(2) 0.0020(2) Br1 0.0169(3) 0.0260(3) 0.0261(3) 0.0027(2) -0.0032(2) -0.0016(2) Br2 0.0252(3) 0.0263(3) 0.0236(3) -0.0049(2) 0.0078(2) 0.0001(2) Br3 0.0249(3) 0.0149(3) 0.0341(3) 0.0042(2) -0.0006(2) -0.0024(2) Br4 0.0208(3) 0.0274(3) 0.0179(3) -0.0042(2) 0.0021(2) 0.0007(2) Br5 0.0242(3) 0.0152(3) 0.0287(3) 0.0038(2) 0.0013(2) -0.0027(2) Br6 0.0182(3) 0.0208(3) 0.0218(3) 0.0007(2) -0.0016(2) -0.0002(2) Br7 0.0461(4) 0.0205(3) 0.0245(3) 0.0029(2) -0.0027(3) 0.0044(3) Br8 0.0224(3) 0.0209(3) 0.0450(4) -0.0014(3) 0.0103(3) 0.0017(2) Br9 0.0259(3) 0.0172(3) 0.0536(4) -0.0037(3) 0.0052(3) -0.0046(3) Br10 0.0538(4) 0.0316(4) 0.0255(3) -0.0103(3) 0.0045(3) -0.0003(3) S1 0.0176(6) 0.0159(7) 0.0187(6) -0.0003(5) -0.0001(5) -0.0011(5) S2A 0.0186(12) 0.0169(12) 0.0189(11) -0.0023(9) -0.0009(9) -0.0011(9) S2B 0.0228(18) 0.0155(18) 0.0167(17) -0.0020(13) 0.0024(13) 0.0010(14) C1 0.031(3) 0.040(4) 0.022(3) -0.014(3) -0.002(3) 0.001(3) C2 0.025(3) 0.023(3) 0.032(3) -0.001(3) -0.002(3) 0.003(3) C3A 0.026(3) 0.022(3) 0.027(3) 0.001(3) -0.001(2) 0.008(3) C4A 0.064(6) 0.039(5) 0.089(7) -0.031(5) -0.053(5) 0.013(4) C3B 0.026(3) 0.022(3) 0.027(3) 0.001(3) -0.001(2) 0.008(3) C4B 0.064(6) 0.039(5) 0.089(7) -0.031(5) -0.053(5) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 Br1 2.4203(7) . ? Nb1 Br3 2.4762(8) . ? Nb1 Br4 2.4775(7) . ? Nb1 Br5 2.4830(8) . ? Nb1 Br2 2.5113(8) . ? Nb1 S1 2.7076(14) . ? Nb2 Br6 2.4301(7) . ? Nb2 Br9 2.4665(9) . ? Nb2 Br10 2.4866(8) . ? Nb2 Br7 2.4879(9) . ? Nb2 Br8 2.4930(8) . ? Nb2 S2A 2.714(2) . ? Nb2 S2B 2.720(4) . ? S1 C2 1.792(6) . ? S1 C1 1.797(6) . ? S2A C4A 1.729(8) . ? S2A C3A 1.801(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Nb1 Br3 97.33(3) . . ? Br1 Nb1 Br4 96.74(3) . . ? Br3 Nb1 Br4 92.02(3) . . ? Br1 Nb1 Br5 96.99(3) . . ? Br3 Nb1 Br5 165.12(3) . . ? Br4 Nb1 Br5 90.28(3) . . ? Br1 Nb1 Br2 97.44(3) . . ? Br3 Nb1 Br2 87.76(3) . . ? Br4 Nb1 Br2 165.73(3) . . ? Br5 Nb1 Br2 86.42(3) . . ? Br1 Nb1 S1 172.90(4) . . ? Br3 Nb1 S1 78.41(4) . . ? Br4 Nb1 S1 77.86(3) . . ? Br5 Nb1 S1 87.72(4) . . ? Br2 Nb1 S1 88.13(4) . . ? Br6 Nb2 Br9 96.54(3) . . ? Br6 Nb2 Br10 98.99(3) . . ? Br9 Nb2 Br10 88.24(3) . . ? Br6 Nb2 Br7 95.93(3) . . ? Br9 Nb2 Br7 167.39(3) . . ? Br10 Nb2 Br7 88.00(3) . . ? Br6 Nb2 Br8 96.11(3) . . ? Br9 Nb2 Br8 91.04(3) . . ? Br10 Nb2 Br8 164.87(3) . . ? Br7 Nb2 Br8 89.46(3) . . ? Br6 Nb2 S2A 166.63(6) . . ? Br9 Nb2 S2A 76.13(5) . . ? Br10 Nb2 S2A 92.03(5) . . ? Br7 Nb2 S2A 91.98(5) . . ? Br8 Nb2 S2A 73.15(5) . . ? Br6 Nb2 S2B 165.80(8) . . ? Br9 Nb2 S2B 94.38(8) . . ? Br10 Nb2 S2B 72.27(8) . . ? Br7 Nb2 S2B 73.01(8) . . ? Br8 Nb2 S2B 92.73(8) . . ? S2A Nb2 S2B 27.30(9) . . ? C2 S1 C1 100.9(3) . . ? C2 S1 Nb1 110.7(2) . . ? C1 S1 Nb1 111.1(2) . . ? C4A S2A C3A 105.4(4) . . ? C4A S2A Nb2 112.2(3) . . ? C3A S2A Nb2 109.8(2) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S2A C3A H3A1 109.5 . . ? S2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? S2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? S2A C4A H4A1 109.5 . . ? S2A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? S2A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # Br1 Nb1 S1 C2 -115.1(4) . . . . ? # Br1 Nb1 S1 C1 133.6(4) . . . . ? Br3 Nb1 S1 C2 -168.8(2) . . . . ? Br4 Nb1 S1 C2 -74.2(2) . . . . ? Br5 Nb1 S1 C2 16.6(2) . . . . ? Br2 Nb1 S1 C2 103.1(2) . . . . ? Br3 Nb1 S1 C1 79.9(3) . . . . ? Br4 Nb1 S1 C1 174.6(3) . . . . ? Br5 Nb1 S1 C1 -94.6(3) . . . . ? Br2 Nb1 S1 C1 -8.2(3) . . . . ? Br6 Nb2 S2A C4A -131.6(4) . . . . ? Br9 Nb2 S2A C4A -73.7(4) . . . . ? Br10 Nb2 S2A C4A 14.0(4) . . . . ? Br7 Nb2 S2A C4A 102.0(4) . . . . ? Br8 Nb2 S2A C4A -169.1(4) . . . . ? S2B Nb2 S2A C4A 56.8(4) . . . . ? Br6 Nb2 S2A C3A 111.5(3) . . . . ? Br9 Nb2 S2A C3A 169.4(2) . . . . ? Br10 Nb2 S2A C3A -102.9(2) . . . . ? Br7 Nb2 S2A C3A -14.9(2) . . . . ? Br8 Nb2 S2A C3A 74.0(2) . . . . ? S2B Nb2 S2A C3A -60.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.064 _refine_diff_density_min -1.317 _refine_diff_density_rms 0.192 #===END OF CIF ============================================================== # 08rj001 data_08rj001 _database_code_depnum_ccdc_archive 'CCDC 723270' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-10-01 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Pentachloro(dimethylselenide-Se)niobium(V) ; # Me2Se names: # dimethylselenide # methylselanylmethane (chemspider) # (methylseleno)methane (iLab (defaults)) _chemical_name_common Pentachloro(dimethylselenide-Se)niobium(V) _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Cl5 Nb Se' _chemical_formula_sum 'C2 H6 Cl5 Nb Se' _chemical_formula_weight 379.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _space_group_IT_number 36 _space_group_name_Hall 'C 2c -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.999(2) _cell_length_b 11.924(3) _cell_length_c 10.796(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1029.7(5) # shelx gives (4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 682 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 5.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7012 # 0.4908 _exptl_absorpt_correction_T_max 1.0000 # 0.5887 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4290 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1179 _reflns_number_gt 1134 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.1511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.075(13) _chemical_absolute_configuration ad _refine_ls_number_reflns 1179 _refine_ls_number_parameters 50 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 1.0000 0.70577(4) 0.26297(4) 0.01802(13) Uani 1 2 d S . . Se1 Se 1.0000 0.93269(5) 0.19060(6) 0.02210(15) Uani 1 2 d S . . Cl1 Cl 1.0000 0.52014(13) 0.31902(16) 0.0336(4) Uani 1 2 d S . . Cl2 Cl 1.0000 0.77958(13) 0.46273(14) 0.0275(3) Uani 1 2 d S . . Cl3 Cl 0.71268(11) 0.73077(9) 0.25934(13) 0.0289(2) Uani 1 1 d . . . Cl4 Cl 1.0000 0.67394(12) 0.05109(13) 0.0251(3) Uani 1 2 d S . . C1 C 0.8193(6) 0.9433(4) 0.0704(5) 0.0283(10) Uani 1 1 d . . . H1A H 0.8296 0.8824 0.0100 0.042 Uiso 1 1 calc R . . H1B H 0.8257 1.0156 0.0276 0.042 Uiso 1 1 calc R . . H1C H 0.7117 0.9372 0.1132 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0198(2) 0.0182(2) 0.0160(2) -0.0003(2) 0.000 0.000 Se1 0.0269(3) 0.0171(3) 0.0222(3) -0.0018(2) 0.000 0.000 Cl1 0.0528(11) 0.0207(7) 0.0271(7) 0.0043(6) 0.000 0.000 Cl2 0.0342(9) 0.0307(8) 0.0176(7) -0.0042(6) 0.000 0.000 Cl3 0.0189(5) 0.0390(5) 0.0287(5) 0.0044(5) 0.0005(5) -0.0030(4) Cl4 0.0352(9) 0.0231(7) 0.0168(6) -0.0019(6) 0.000 0.000 C1 0.029(3) 0.023(2) 0.033(3) 0.0061(18) -0.004(2) 0.0009(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 Cl1 2.2947(16) . ? Nb1 Cl3 2.3178(11) 4_755 ? Nb1 Cl3 2.3178(11) . ? Nb1 Cl4 2.3187(16) . ? Nb1 Cl2 2.3293(16) . ? Nb1 Se1 2.8163(9) . ? Se1 C1 1.946(5) . ? Se1 C1 1.946(5) 4_755 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Nb1 Cl3 97.38(3) . 4_755 ? Cl1 Nb1 Cl3 97.38(3) . . ? Cl3 Nb1 Cl3 165.09(6) 4_755 . ? Cl1 Nb1 Cl4 95.87(6) . . ? Cl3 Nb1 Cl4 90.25(4) 4_755 . ? Cl3 Nb1 Cl4 90.25(4) . . ? Cl1 Nb1 Cl2 96.91(6) . . ? Cl3 Nb1 Cl2 88.11(4) 4_755 . ? Cl3 Nb1 Cl2 88.11(4) . . ? Cl4 Nb1 Cl2 167.22(6) . . ? Cl1 Nb1 Se1 179.18(5) . . ? Cl3 Nb1 Se1 82.63(3) 4_755 . ? Cl3 Nb1 Se1 82.63(3) . . ? Cl4 Nb1 Se1 83.31(4) . . ? Cl2 Nb1 Se1 83.91(4) . . ? C1 Se1 C1 95.9(3) . 4_755 ? C1 Se1 Nb1 104.32(14) . . ? C1 Se1 Nb1 104.32(14) 4_755 . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # Cl1 Nb1 Se1 C1 50.03(17) . . . . ? # Cl1 Nb1 Se1 C1 -50.03(17) . . . 4_755 ? Cl3 Nb1 Se1 C1 141.16(17) 4_755 . . . ? Cl3 Nb1 Se1 C1 -41.09(17) . . . . ? Cl4 Nb1 Se1 C1 50.03(16) . . . . ? Cl2 Nb1 Se1 C1 -129.97(16) . . . . ? Cl3 Nb1 Se1 C1 41.09(17) 4_755 . . 4_755 ? Cl3 Nb1 Se1 C1 -141.16(17) . . . 4_755 ? Cl4 Nb1 Se1 C1 -50.03(16) . . . 4_755 ? Cl2 Nb1 Se1 C1 129.97(16) . . . 4_755 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.651 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.109 #===END OF CIF ============================================================== # 08mj03 data_08mj03b _database_code_depnum_ccdc_archive 'CCDC 723271' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-04 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,2-bis(methylthiomethyl)benzenebis(pentachloroniobium(V)) ; _chemical_name_common 1,2-bis(methylthiomethyl)benzenebis(pentachloroniobium(V)) _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 Cl10 Nb2 S2' _chemical_formula_sum 'C10 H14 Cl10 Nb2 S2' _chemical_formula_structural '(C10 H14 S2) (Cl5 Nb)2' _chemical_formula_weight 738.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n c 2' _symmetry_Int_Tables_number 30 # Superceded ** _symmetry_space_group_name_Hall 'P 2 -2bc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' _cell_length_a 10.3087(5) _cell_length_b 22.4368(15) _cell_length_c 10.3102(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2384.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2981 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1961 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15435 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4956 _reflns_number_gt 4635 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+13.3821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0055(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(9) _chemical_absolute_configuration ad _refine_ls_number_reflns 4956 _refine_ls_number_parameters 218 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.93651(5) 0.14378(2) 0.33980(6) 0.02651(16) Uani 1 1 d . . . Nb2 Nb 0.40173(6) 0.15017(3) 0.85872(7) 0.03472(19) Uani 1 1 d . . . Cl1 Cl 0.9006(2) 0.17143(9) 0.1306(2) 0.0434(5) Uani 1 1 d . . . Cl2 Cl 1.1099(2) 0.20664(10) 0.3829(3) 0.0624(8) Uani 1 1 d . . . Cl3 Cl 1.0826(2) 0.06755(10) 0.2959(2) 0.0483(6) Uani 1 1 d . . . Cl4 Cl 0.77387(14) 0.07337(6) 0.35137(19) 0.0300(3) Uani 1 1 d . . . Cl5 Cl 0.7989(2) 0.21111(9) 0.4374(2) 0.0468(5) Uani 1 1 d . . . Cl6 Cl 0.3019(3) 0.18541(13) 0.6793(2) 0.0591(7) Uani 1 1 d . . . Cl7 Cl 0.22431(19) 0.15486(13) 0.9948(2) 0.0554(6) Uani 1 1 d . . . Cl8 Cl 0.3600(5) 0.05032(12) 0.8247(3) 0.1191(18) Uani 1 1 d . . . Cl9 Cl 0.6034(3) 0.13667(15) 0.7636(3) 0.0935(14) Uani 1 1 d . . . Cl10 Cl 0.4732(2) 0.24012(9) 0.9368(3) 0.0507(6) Uani 1 1 d . . . S1 S 1.00289(16) 0.10744(7) 0.58092(19) 0.0267(3) Uani 1 1 d . . . S2 S 0.52272(17) 0.10440(9) 1.0717(2) 0.0368(4) Uani 1 1 d . . . C1 C 0.9645(10) 0.1657(4) 0.6964(9) 0.047(2) Uani 1 1 d . . . H1A H 1.0167 0.2011 0.6773 0.070 Uiso 1 1 calc R . . H1B H 0.9839 0.1517 0.7843 0.070 Uiso 1 1 calc R . . H1C H 0.8722 0.1757 0.6900 0.070 Uiso 1 1 calc R . . C2 C 0.8970(6) 0.0469(3) 0.6360(6) 0.0237(13) Uani 1 1 d . . . H2A H 0.8083 0.0624 0.6503 0.028 Uiso 1 1 calc R . . H2B H 0.8926 0.0156 0.5686 0.028 Uiso 1 1 calc R . . C3 C 0.9482(8) 0.0208(3) 0.7596(7) 0.0313(16) Uani 1 1 d . . . C4 C 0.9001(10) 0.0408(4) 0.8783(8) 0.046(2) Uani 1 1 d . . . H4 H 0.8316 0.0691 0.8795 0.055 Uiso 1 1 calc R . . C5 C 0.9506(12) 0.0202(4) 0.9949(8) 0.059(3) Uani 1 1 d . . . H5 H 0.9161 0.0342 1.0748 0.071 Uiso 1 1 calc R . . C6 C 0.5232(8) 0.1625(4) 1.1936(10) 0.042(2) Uani 1 1 d . . . H6A H 0.5823 0.1944 1.1669 0.064 Uiso 1 1 calc R . . H6B H 0.5522 0.1459 1.2765 0.064 Uiso 1 1 calc R . . H6C H 0.4354 0.1786 1.2032 0.064 Uiso 1 1 calc R . . C7 C 0.4092(7) 0.0514(4) 1.1443(9) 0.0391(19) Uani 1 1 d . . . H7A H 0.3260 0.0720 1.1615 0.047 Uiso 1 1 calc R . . H7B H 0.3920 0.0190 1.0815 0.047 Uiso 1 1 calc R . . C8 C 0.4576(10) 0.0250(4) 1.2672(8) 0.046(2) Uani 1 1 d U . . C9 C 0.4208(13) 0.0482(6) 1.3859(11) 0.088(5) Uani 1 1 d U . . H9 H 0.3653 0.0820 1.3871 0.106 Uiso 1 1 calc R . . C10 C 0.460(2) 0.0252(7) 1.5000(9) 0.147(11) Uani 1 1 d U . . H10 H 0.4342 0.0429 1.5794 0.176 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0231(3) 0.0219(3) 0.0345(4) 0.0079(3) -0.0031(3) 0.00105(19) Nb2 0.0351(3) 0.0317(3) 0.0374(4) -0.0072(3) 0.0130(3) -0.0006(2) Cl1 0.0540(12) 0.0411(11) 0.0350(10) 0.0160(8) -0.0002(9) 0.0069(9) Cl2 0.0452(11) 0.0518(12) 0.090(2) 0.0429(12) -0.0299(12) -0.0282(9) Cl3 0.0401(11) 0.0508(12) 0.0540(13) 0.0189(9) 0.0214(9) 0.0207(9) Cl4 0.0258(7) 0.0281(7) 0.0360(9) 0.0033(7) -0.0085(8) -0.0037(5) Cl5 0.0508(11) 0.0335(10) 0.0562(12) -0.0172(9) -0.0227(10) 0.0209(8) Cl6 0.0604(14) 0.0801(17) 0.0368(11) 0.0017(11) -0.0051(10) -0.0247(13) Cl7 0.0227(9) 0.107(2) 0.0363(11) 0.0080(11) 0.0058(8) 0.0072(10) Cl8 0.272(5) 0.0467(14) 0.0386(14) -0.0174(10) 0.055(2) -0.061(2) Cl9 0.086(2) 0.093(2) 0.101(2) 0.0512(19) 0.071(2) 0.0570(18) Cl10 0.0551(12) 0.0301(9) 0.0669(15) -0.0001(9) -0.0219(11) -0.0027(8) S1 0.0267(8) 0.0194(7) 0.0339(8) 0.0008(6) -0.0093(7) -0.0006(6) S2 0.0244(8) 0.0323(9) 0.0537(12) 0.0036(8) 0.0114(8) 0.0064(7) C1 0.068(6) 0.028(4) 0.044(5) -0.012(3) -0.026(4) 0.009(4) C2 0.026(3) 0.023(3) 0.022(3) 0.002(2) 0.002(3) -0.002(2) C3 0.050(4) 0.020(3) 0.023(3) 0.002(3) -0.001(3) 0.010(3) C4 0.070(6) 0.042(4) 0.024(4) 0.001(3) -0.001(4) 0.026(4) C5 0.099(8) 0.056(6) 0.022(4) -0.003(4) 0.007(5) 0.044(6) C6 0.028(4) 0.033(4) 0.066(6) 0.001(4) -0.011(4) 0.000(3) C7 0.022(3) 0.038(4) 0.057(5) 0.003(4) 0.017(3) 0.000(3) C8 0.064(6) 0.046(5) 0.027(3) -0.011(3) 0.014(4) -0.030(4) C9 0.102(9) 0.099(8) 0.063(7) -0.059(6) 0.053(6) -0.078(7) C10 0.22(2) 0.200(19) 0.023(3) -0.042(6) 0.045(7) -0.182(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 Cl1 2.275(2) . ? Nb1 Cl5 2.303(2) . ? Nb1 Cl4 2.3067(15) . ? Nb1 Cl2 2.320(2) . ? Nb1 Cl3 2.323(2) . ? Nb1 S1 2.7043(19) . ? Nb2 Cl6 2.260(3) . ? Nb2 Cl10 2.295(2) . ? Nb2 Cl7 2.308(2) . ? Nb2 Cl8 2.308(2) . ? Nb2 Cl9 2.318(3) . ? Nb2 S2 2.726(2) . ? S1 C1 1.811(8) . ? S1 C2 1.832(6) . ? S2 C6 1.810(9) . ? S2 C7 1.828(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.498(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.395(10) . ? C3 C3 1.420(14) 2_755 ? C4 C5 1.389(11) . ? C4 H4 0.9500 . ? C5 C5 1.362(18) 2_755 ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.485(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.383(12) . ? C8 C8 1.42(2) 2_655 ? C9 C10 1.35(2) . ? C9 H9 0.9500 . ? C10 C10 1.39(5) 2_655 ? C10 H10 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Nb1 Cl5 97.77(8) . . ? Cl1 Nb1 Cl4 96.76(8) . . ? Cl5 Nb1 Cl4 88.80(7) . . ? Cl1 Nb1 Cl2 98.11(9) . . ? Cl5 Nb1 Cl2 89.55(10) . . ? Cl4 Nb1 Cl2 165.13(8) . . ? Cl1 Nb1 Cl3 96.97(8) . . ? Cl5 Nb1 Cl3 165.24(9) . . ? Cl4 Nb1 Cl3 88.68(7) . . ? Cl2 Nb1 Cl3 89.16(9) . . ? Cl1 Nb1 S1 174.31(7) . . ? Cl5 Nb1 S1 87.25(7) . . ? Cl4 Nb1 S1 85.98(6) . . ? Cl2 Nb1 S1 79.18(7) . . ? Cl3 Nb1 S1 78.06(7) . . ? Cl6 Nb2 Cl10 97.22(9) . . ? Cl6 Nb2 Cl7 96.96(9) . . ? Cl10 Nb2 Cl7 90.06(10) . . ? Cl6 Nb2 Cl8 97.50(13) . . ? Cl10 Nb2 Cl8 165.23(13) . . ? Cl7 Nb2 Cl8 89.36(13) . . ? Cl6 Nb2 Cl9 96.19(12) . . ? Cl10 Nb2 Cl9 88.58(13) . . ? Cl7 Nb2 Cl9 166.85(11) . . ? Cl8 Nb2 Cl9 88.64(15) . . ? Cl6 Nb2 S2 178.28(9) . . ? Cl10 Nb2 S2 84.36(8) . . ? Cl7 Nb2 S2 83.68(7) . . ? Cl8 Nb2 S2 80.91(12) . . ? Cl9 Nb2 S2 83.17(10) . . ? C1 S1 C2 101.6(4) . . ? C1 S1 Nb1 109.4(3) . . ? C2 S1 Nb1 111.0(2) . . ? C6 S2 C7 100.7(4) . . ? C6 S2 Nb2 106.8(3) . . ? C7 S2 Nb2 106.4(3) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 110.1(5) . . ? C3 C2 H2A 109.6 . . ? S1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? S1 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C3 118.6(4) . 2_755 ? C4 C3 C2 119.7(6) . . ? C3 C3 C2 121.5(4) 2_755 . ? C5 C4 C3 121.3(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C5 C5 C4 120.1(5) 2_755 . ? C5 C5 H5 120.0 2_755 . ? C4 C5 H5 120.0 . . ? S2 C6 H6A 109.5 . . ? S2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 S2 113.2(6) . . ? C8 C7 H7A 108.9 . . ? S2 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? S2 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C8 117.7(9) . 2_655 ? C9 C8 C7 120.8(11) . . ? C8 C8 C7 121.4(5) 2_655 . ? C10 C9 C8 123.0(16) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C10 119.2(10) . 2_655 ? C9 C10 H10 120.4 . . ? C10 C10 H10 120.4 2_655 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.102 _refine_diff_density_min -1.561 _refine_diff_density_rms 0.147 #===END OF CIF ============================================================== # 08mj29 data_08mj29 _database_code_depnum_ccdc_archive 'CCDC 723272' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-30 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (2,5-diselenahexane-Se,Se')bis(pentachloroniobium(V)) ; # I-Lab gave Se ligand as 1,2-bis(methylseleno)ethane _chemical_name_common (2,5-diselenahexane-Se,Se')bis(pentachloroniobium(V)) _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Cl10 Nb2 Se2' _chemical_formula_sum 'C4 H10 Cl10 Nb2 Se2' _chemical_formula_structural '(C4 H10 Se2) (Cl5 Nb)2' _chemical_formula_weight 756.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9033(15) _cell_length_b 13.020(4) _cell_length_c 11.111(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.812(15) _cell_angle_gamma 90.00 _cell_volume 986.9(5) # (4) from shelxl _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 33108 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 6.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6491 # 0.5768 _exptl_absorpt_correction_T_max 1.0000 # 0.8863 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17501 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 27.70 _reflns_number_total 2267 _reflns_number_gt 1599 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+14.0255P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2267 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.06348(11) 0.75799(6) 0.39968(7) 0.0223(2) Uani 1 1 d . . . Se1 Se 0.41445(12) 0.64986(6) 0.39162(8) 0.0220(2) Uani 1 1 d . . . Cl1 Cl -0.2108(3) 0.85611(18) 0.3969(2) 0.0315(5) Uani 1 1 d . . . Cl2 Cl 0.2859(3) 0.88184(17) 0.4825(2) 0.0317(5) Uani 1 1 d . . . Cl3 Cl 0.0756(3) 0.68695(18) 0.5921(2) 0.0313(5) Uani 1 1 d . . . Cl4 Cl -0.0878(3) 0.60806(17) 0.3183(2) 0.0312(5) Uani 1 1 d . . . Cl5 Cl 0.1243(3) 0.80167(18) 0.2052(2) 0.0297(5) Uani 1 1 d . . . C1 C 0.3757(14) 0.5799(8) 0.2347(8) 0.031(2) Uani 1 1 d . . . H1A H 0.4822 0.5306 0.2319 0.047 Uiso 1 1 calc R . . H1B H 0.3754 0.6305 0.1693 0.047 Uiso 1 1 calc R . . H1C H 0.2500 0.5435 0.2239 0.047 Uiso 1 1 calc R . . C2 C 0.4015(12) 0.5279(6) 0.4925(8) 0.026(2) Uani 1 1 d . . . H2A H 0.3706 0.5481 0.5733 0.031 Uiso 1 1 calc R . . H2B H 0.2965 0.4816 0.4535 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0234(4) 0.0199(4) 0.0242(4) 0.0011(3) 0.0052(3) 0.0022(3) Se1 0.0225(4) 0.0180(4) 0.0263(5) 0.0015(4) 0.0061(3) 0.0012(4) Cl1 0.0305(12) 0.0306(12) 0.0337(13) 0.0000(10) 0.0058(10) 0.0109(10) Cl2 0.0342(12) 0.0249(11) 0.0346(13) -0.0046(10) 0.0010(10) 0.0007(9) Cl3 0.0345(12) 0.0347(12) 0.0264(12) 0.0076(10) 0.0101(9) 0.0093(10) Cl4 0.0272(11) 0.0281(12) 0.0386(14) -0.0035(10) 0.0060(10) -0.0038(9) Cl5 0.0340(12) 0.0283(12) 0.0276(12) 0.0071(10) 0.0078(9) 0.0038(9) C1 0.039(5) 0.037(5) 0.017(5) 0.005(4) 0.006(4) 0.005(4) C2 0.027(5) 0.021(4) 0.031(5) 0.000(4) 0.008(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 Cl1 2.280(2) . ? Nb1 Cl2 2.318(2) . ? Nb1 Cl3 2.319(2) . ? Nb1 Cl4 2.330(2) . ? Nb1 Cl5 2.334(2) . ? Nb1 Se1 2.8155(12) . ? Se1 C2 1.954(9) . ? Se1 C1 1.949(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C2 1.527(17) 3_666 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Nb1 Cl2 96.54(9) . . ? Cl1 Nb1 Cl3 98.54(9) . . ? Cl2 Nb1 Cl3 89.05(9) . . ? Cl1 Nb1 Cl4 98.18(9) . . ? Cl2 Nb1 Cl4 165.28(9) . . ? Cl3 Nb1 Cl4 88.53(9) . . ? Cl1 Nb1 Cl5 96.76(9) . . ? Cl2 Nb1 Cl5 89.76(9) . . ? Cl3 Nb1 Cl5 164.69(9) . . ? Cl4 Nb1 Cl5 88.76(9) . . ? Cl1 Nb1 Se1 175.20(7) . . ? Cl2 Nb1 Se1 80.76(7) . . ? Cl3 Nb1 Se1 85.42(6) . . ? Cl4 Nb1 Se1 84.58(6) . . ? Cl5 Nb1 Se1 79.32(6) . . ? C2 Se1 C1 97.0(4) . . ? C2 Se1 Nb1 105.9(2) . . ? C1 Se1 Nb1 105.1(3) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C2 Se1 109.3(7) 3_666 . ? C2 C2 H2A 109.8 3_666 . ? Se1 C2 H2A 109.8 . . ? C2 C2 H2B 109.8 3_666 . ? Se1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # Cl1 Nb1 Se1 C2 175.5(9) . . . . ? # Cl1 Nb1 Se1 C1 -82.6(9) . . . . ? Cl2 Nb1 Se1 C2 119.5(3) . . . . ? Cl3 Nb1 Se1 C2 29.7(3) . . . . ? Cl4 Nb1 Se1 C2 -59.2(3) . . . . ? Cl5 Nb1 Se1 C2 -149.0(3) . . . . ? Cl2 Nb1 Se1 C1 -138.5(3) . . . . ? Cl3 Nb1 Se1 C1 131.7(3) . . . . ? Cl4 Nb1 Se1 C1 42.7(3) . . . . ? Cl5 Nb1 Se1 C1 -47.0(3) . . . . ? C1 Se1 C2 C2 79.8(9) . . . 3_666 ? Nb1 Se1 C2 C2 -172.2(8) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.985 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.250 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================